CN107164094A - Hyperchromic flavouring proline maillard reaction thing preparation method and applications - Google Patents
Hyperchromic flavouring proline maillard reaction thing preparation method and applications Download PDFInfo
- Publication number
- CN107164094A CN107164094A CN201710549540.9A CN201710549540A CN107164094A CN 107164094 A CN107164094 A CN 107164094A CN 201710549540 A CN201710549540 A CN 201710549540A CN 107164094 A CN107164094 A CN 107164094A
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- proline
- maillard
- enhancing
- aroma
- sugar
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Classifications
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- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/0003—Compounds of unspecified constitution defined by the chemical reaction for their preparation
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- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B3/00—Preparing tobacco in the factory
- A24B3/12—Steaming, curing, or flavouring tobacco
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
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Abstract
Description
技术领域technical field
本发明涉及烟用添加剂技术领域,具体是一种增色增香脯氨酸美拉德反应物制备方法及其应用。The invention relates to the technical field of cigarette additives, in particular to a preparation method and application of proline-Maillard reactants for color enhancement and aroma enhancement.
背景技术Background technique
美拉德反应类香料一直是烟草和食品上极为重要和极有应用价值的香料,美拉德反应物在烟用香料中应用广泛。烟草在调制、陈化、加工和燃吸等过程中,均可能发生美拉德反应。随着人们健康意识的提高,烟厂在解决降低卷烟焦油量、而又能保持或满足卷烟吸食可用性方面所面临的困难日益突出。美拉德反应作为烟草特征香气形成的重要途径之一,在烟草增香中的应用研究倍受青睐。反应产生的香气根据糖源、氮源不同也不同,反应产生大量杂环香味化合物,对卷烟烟气有改善作用。Maillard reaction flavors have always been extremely important and valuable flavors in tobacco and food, and Maillard reactants are widely used in tobacco flavors. Maillard reactions may occur in tobacco during the process of conditioning, aging, processing and smoking. With the improvement of people's health awareness, the difficulties faced by cigarette factories in solving the problem of reducing the amount of cigarette tar while maintaining or satisfying the availability of cigarette smoking have become increasingly prominent. As one of the important ways to form the characteristic aroma of tobacco, the Maillard reaction has been favored for its application in tobacco flavoring. The aroma produced by the reaction is also different according to the sugar source and nitrogen source, and a large amount of heterocyclic aroma compounds are produced by the reaction, which can improve the smoke of cigarettes.
再造烟叶可作为烟制品原料,用来代替天然的雪茄内包叶,现已广泛用作卷烟原料。雪茄型卷烟是融合雪茄烟和烤烟的优势特征,形成兼具雪茄烟浓郁丰盈和烤烟纯净舒适的风味特色,构建出不同于雪茄型和烤烟型的现代经典中式雪茄品类。现有技术中,普通卷烟纸(茄衣)只是起到包裹烟丝、提供外观视觉效果的作用,通常情况下,为满足高速卷烟机的正常运行,对卷烟纸生产重点是从物理性能上考虑,在原料的选择上采用的是全商品浆板;在生产工艺上,通过控制不同原料配比及打浆度和在卷烟纸生产过程中加入适量碳酸钙和助燃剂来达到物理指标和燃烧性能的要求;但这些对卷烟品质的提高是较为有限的。众所周知,所谓吸烟其实就是抽吸烟丝燃烧后产生的烟气,而其中茄衣却是烟丝的载体,卷烟纸与其它卷烟材料所不同的是,它将参与卷烟燃烧,而现有技术采用的全商品浆板生产的卷烟纸,存在卷烟燃烧过程中产生较多木质气、刺辣感而影响卷烟烟气清纯气味的问题。Reconstituted tobacco can be used as a raw material for tobacco products to replace natural cigar wrappers, and has been widely used as a raw material for cigarettes. Cigar-shaped cigarettes combine the advantages of cigars and flue-cured tobacco to form a rich and full-bodied cigar and pure and comfortable flavor characteristics of flue-cured tobacco, creating a modern classic Chinese cigar category that is different from cigars and flue-cured tobacco. In the prior art, ordinary cigarette paper (wrapper) only plays the role of wrapping shredded tobacco and providing appearance and visual effects. Usually, in order to meet the normal operation of high-speed cigarette machines, the focus of cigarette paper production is to consider physical properties. In the selection of raw materials, all-commercial pulp board is used; in the production process, the requirements of physical indicators and combustion performance are met by controlling the ratio of different raw materials and beating degree and adding appropriate amount of calcium carbonate and combustion improver in the production process of cigarette paper. ; But these are comparatively limited to the improvement of cigarette quality. As we all know, the so-called smoking is actually the smoke produced after the shredded tobacco is burned, and the wrapper is the carrier of the shredded tobacco. The difference between cigarette paper and other cigarette materials is that it will participate in the burning of cigarettes. Cigarette paper produced from commercial pulp boards has the problem of producing more woody gas and pungent sensation during the burning process of cigarettes, which affects the pure smell of cigarette smoke.
合成色素色泽鲜艳,着色力强,色调多样,但它有一个大缺点,即具毒性(包括毒性、致泻性和致癌性)。天然色素因色调与食品天然色调接近、安全性比合成色素可靠等优点而受到普遍的重视和广泛的研究。利用美拉德反应生成的香料在国际上认为是属于天然香料范畴,被美国食品药品管理局(FDA)认定为是一般公认安全的产品(GRAS)。Synthetic pigments are bright in color, strong in coloring power, and diverse in hue, but they have a major disadvantage, that is, they are toxic (including toxicity, diarrhea, and carcinogenicity). Natural pigments have been widely valued and extensively studied because of their advantages such as the color close to the natural color of food and the safety and reliability compared with synthetic pigments. The spices produced by the Maillard reaction are internationally considered to belong to the category of natural flavors, and are recognized as generally recognized as safe products (GRAS) by the US Food and Drug Administration (FDA).
公开号为CN101411543的中国专利申请,公开了一种制备烟用香料的方法,其将糖类物质与氨基酸进行反应,制得烟用香料。该方法采用糖类与氨基酸间的美拉德反应产物作为烟用香料,具有增香的作用。公开号为CN101637305A的中国专利申请,公开了一种利用美拉德反应制备烟用香料的方法,其将葡萄糖、复配氨基酸及特种定向增香型烟末浸膏进行反应,具有巧克力和烤香的烟用香料等。该方法原料来源复杂,成本较高,制得香料香型较单一,难于普遍应用于卷烟中。其他复合糖源、氮源的美拉德反应香料,原料来源复杂,成本较高,制备的美拉德反应物成分较复杂,难以纯化,引起烟气的刺激性较大。授权发明专利ZL201310268308.X公开了一种调控美拉德反应制备烟用香料的方法,其将氨基酸与葡萄糖按照质量比为1:2~1:6混合溶解于水中得到起始混合液,起始混合液中葡萄糖的质量浓度为10%~20%,pH8~12,温度控制在105℃~120℃反应0.5~1小时;添加L-抗坏血酸,105℃~120℃下继续反应0.5~1小时,制得美拉德反应型烟用香料,该美拉德反应香料存在多糖含量高、成分复杂、粘度大、吸潮性强、几乎没有着色能力的缺陷。目前已有的脯氨酸美拉德反应物的报道为丙二醇/水体系,氨基酸和糖通常比例为1:2~1:1.2,催化剂为氨水、羟基丁基茴香醚或特丁基对苯二酚等,其反应物应用时具有多糖含量高、吸潮性大的缺陷,而已知的脯氨酸美拉德反应物的报道中,其酸值不高,且未见脯氨酸美拉德反应物增色增香、改善再造烟叶及其茄衣的外观和感官品质的报道。The Chinese patent application with publication number CN101411543 discloses a method for preparing tobacco flavors, which involves reacting carbohydrates with amino acids to prepare tobacco flavors. In the method, the Maillard reaction product between sugar and amino acid is used as the flavor for tobacco, which has the effect of increasing flavor. The Chinese patent application with the publication number CN101637305A discloses a method for preparing tobacco flavors by using the Maillard reaction. It reacts glucose, compound amino acids and special directional flavor-enhancing tobacco powder extract, which has chocolate and roasted flavors. Tobacco spices, etc. The source of raw materials in this method is complicated, the cost is relatively high, and the flavor type of the prepared spice is relatively single, so it is difficult to be widely used in cigarettes. Other Maillard reaction spices with complex sugar sources and nitrogen sources have complex sources of raw materials and high costs. The prepared Maillard reaction products have complex components, are difficult to purify, and cause greater irritation to smoke. Authorized invention patent ZL201310268308.X discloses a method for preparing tobacco flavor by regulating the Maillard reaction, in which amino acid and glucose are mixed and dissolved in water at a mass ratio of 1:2 to 1:6 to obtain an initial mixed solution. The mass concentration of glucose in the mixed solution is 10% to 20%, the pH is 8 to 12, and the temperature is controlled at 105°C to 120°C for 0.5 to 1 hour; add L-ascorbic acid and continue to react at 105°C to 120°C for 0.5 to 1 hour. The Maillard reaction flavor for tobacco is prepared, and the Maillard reaction flavor has the defects of high polysaccharide content, complex components, high viscosity, strong moisture absorption and almost no coloring ability. The existing proline Maillard reactants are reported as propylene glycol/water system, the ratio of amino acid and sugar is usually 1:2~1:1.2, and the catalyst is ammonia water, hydroxybutyl anisole or tert-butyl terephthalate Phenol, etc., the reactant has the defects of high polysaccharide content and high moisture absorption when it is applied, and in the report of the known proline Maillard reactant, its acid value is not high, and there is no proline Maillard Reports on the color and aroma of the reactants, and the improvement of the appearance and sensory qualities of reconstituted tobacco leaves and their wrappers.
发明内容Contents of the invention
本发明的目的是提供一种增色增香脯氨酸美拉德反应物的制备方法及其应用,采用水溶液反应体系,在美拉德反应罐中添加一定比例的脯氨酸、还原糖和反应催化剂,在一定的反应温度、时间、pH条件下进行美拉德反应,工业生产增色增香的脯氨酸美拉德反应物,提高了脯氨酸美拉德反应物的酸值,降低了其吸潮性等缺陷,在再造烟叶及其茄衣中应用,改善其外观和感官品质,协调烟气,使烟气柔和细腻,降低烟气刺激性,改善感官质量,并使其外观接近于雪茄烟外观颜色,自然均匀,工艺条件温和易操作,成本低廉。The object of the present invention is to provide a kind of preparation method and application of proline Maillard reactant of color and aroma enhancement, adopt aqueous solution reaction system, add a certain proportion of proline, reducing sugar and reaction in Maillard reaction tank Catalyst, carry out Maillard reaction under certain reaction temperature, time, pH condition, the proline Maillard reactant of industrial production color enhancement, has improved the acid value of proline Maillard reactant, has reduced Its moisture absorption and other defects are applied in reconstituted tobacco leaves and their wrappers to improve their appearance and sensory quality, coordinate the smoke, make the smoke soft and delicate, reduce the irritation of the smoke, improve the sensory quality, and make the appearance close to The appearance and color of cigars are natural and uniform, the process conditions are mild and easy to operate, and the cost is low.
本发明通过以下技术方案实现:The present invention is realized through the following technical solutions:
一种增色增香脯氨酸美拉德反应物的制备方法,包括如下步骤:A kind of preparation method of proline Maillard reactant of color-enhancing and aroma-enhancing, comprises the steps:
(1)原料准备;准备美拉德反应底物、催化剂和水,其中美拉德反应底物为脯氨酸与糖源,糖源为还原糖或者复合糖源,复合糖源为咖啡豆提取物或还原糖与发酵咖啡豆提取物的复配物;糖源为还原糖时,脯氨酸与还原糖的摩尔比2~8:1,糖源为复合糖源时,脯氨酸与复合糖源的质量比为2~5:1,催化剂占美拉德反应底物质量的0.2~6%,水与反应底物的质量比为1~10:1;(1) Raw material preparation; prepare the Maillard reaction substrate, catalyst and water, wherein the Maillard reaction substrate is proline and sugar source, the sugar source is reducing sugar or complex sugar source, and the complex sugar source is coffee bean extraction compound of reducing sugar and fermented coffee bean extract; when the sugar source is reducing sugar, the molar ratio of proline to reducing sugar is 2 to 8:1; when the sugar source is complex sugar source, the proline and compound The mass ratio of the sugar source is 2-5:1, the catalyst accounts for 0.2-6% of the mass of the Maillard reaction substrate, and the mass ratio of water to the reaction substrate is 1-10:1;
(2)工业生产:先将水加入反应罐中,启动搅拌电机,加热至50~60℃,依次按一定比例加入脯氨酸、糖源,充分搅拌,直至完全溶解后,再加入催化剂;反应过程中,设置美拉德反应罐工艺条件为温度92~180℃,搅拌电机保持开启状态,反应时间为3~24h;(2) Industrial production: first add water to the reaction tank, start the stirring motor, heat to 50-60°C, add proline and sugar source in a certain proportion in turn, stir fully, and then add the catalyst until completely dissolved; During the process, the process conditions of the Maillard reaction tank are set at a temperature of 92-180°C, the stirring motor is kept on, and the reaction time is 3-24 hours;
(3)成品:反应结束后,待反应物在反应罐中自然冷却至35~40℃,过80~100目筛网过滤,以25+0.1公斤/桶的规格灌装,常温避光保存。(3) Finished product: After the reaction, the reactant is naturally cooled to 35-40°C in the reaction tank, filtered through a sieve of 80-100 mesh, filled with a specification of 25+0.1 kg/barrel, and stored at room temperature and protected from light.
进一步的,所述的发酵咖啡豆提取物的制备方法为:咖啡豆粗粉与水的质量比为1:10~50,由龙胆二糖酶、内切纤维素酶、外切纤维素酶、中性和碱性蛋白酶、活性生香鲁氏干酵母按照质量比0.1~0.3:0.5~1:0.5~1:0.5~2:0.5~1:0.5~1,搅拌均匀,对咖啡豆粗粉进行复合发酵,发酵条件为pH6~10、28~38℃、时间2~12h然后90~95℃恒温水浴回流提取1~3次,合并滤液,减压浓缩至相对密度为1.1~1.3,即制得所述发酵咖啡豆提取物。Further, the preparation method of the fermented coffee bean extract is as follows: the mass ratio of coffee bean coarse powder to water is 1:10-50, and gentiobiase, endocellulase, exocellulase , neutral and alkaline proteases, and active dry yeast Luxie rosacei according to the mass ratio of 0.1-0.3:0.5-1:0.5-1:0.5-2:0.5-1:0.5-1, stir evenly, and add coffee beans to the coarse powder Carry out compound fermentation, the fermentation conditions are pH 6-10, 28-38°C, time 2-12h, then 90-95°C constant temperature water bath reflux extraction 1-3 times, combine the filtrate, concentrate under reduced pressure to a relative density of 1.1-1.3, ready-made Obtain the fermented coffee bean extract.
进一步的,所述活性生香鲁氏干酵母和酶均为食品级,龙胆二糖酶的酶活为100~10000u/g,内切纤维素酶、外切纤维素酶、中性和碱性蛋白酶的酶活为2万~20万u/g,复合酶和活性生香鲁氏干酵母占咖啡豆粗粉质量的0.1~0.5%。Further, the active dry yeast and enzymes are food grade, the enzyme activity of gentiobiase is 100-10000u/g, endocellulase, exocellulase, neutral and alkali The enzymatic activity of the protease is 20,000-200,000 u/g, and the compound enzyme and active Dried yeast rushii account for 0.1-0.5% of the mass of the coffee bean meal.
进一步的,所述的复合糖源为还原糖与发酵咖啡豆提取物的复配物时,还原糖总量与发酵咖啡豆提取物质量比为1:1,若还原糖有两种或两种以上,每种还原糖之间为等质量比。Further, when the complex sugar source is a compound of reducing sugar and fermented coffee bean extract, the mass ratio of the total amount of reducing sugar to fermented coffee bean extract is 1:1, if there are two or two kinds of reducing sugar Above, each kind of reducing sugar is equal mass ratio.
进一步的,所述的还原糖为葡萄糖、木糖、半乳糖、阿拉伯糖、麦芽糖、白砂糖、红糖、焦糖、玉米糖浆中的一种或任意几种的组合,均为食品级以上。Further, the reducing sugar is one or any combination of glucose, xylose, galactose, arabinose, maltose, white sugar, brown sugar, caramel, and corn syrup, all of which are above food grade.
进一步的,所述的催化剂为氨水、α-甲基苯甲醛、甲醛、乙醛、丙醛、异戊醛、维生素C中的一种或几种。Further, the catalyst is one or more of ammonia water, α-methylbenzaldehyde, formaldehyde, acetaldehyde, propionaldehyde, isovaleraldehyde, and vitamin C.
本发明还提供一种增色增香脯氨酸美拉德反应物在再造烟叶中的应用,在再造烟叶进行涂布工序时添加,添加量为0.05~1%,能改善再造烟叶的外观和感官品质,与烟气协调,降低烟气刺激性,丰富烟气,使外观色泽接近雪茄烟,自然均匀。The present invention also provides an application of proline Maillard reactant for color enhancement and aroma enhancement in reconstituted tobacco leaves, which is added during the coating process of reconstituted tobacco leaves, and the addition amount is 0.05-1%, which can improve the appearance and sense of reconstituted tobacco leaves Quality, coordinated with the smoke, reducing the irritation of the smoke, enriching the smoke, making the appearance and color close to cigar smoke, natural and uniform.
本发明还提供一种增色增香脯氨酸美拉德反应物在茄衣中的应用,涂布添加量为2~12%,能改善茄衣的外观和感官品质,与烟气协调,降低烟气刺激性,丰富烟气,使外观色泽接近雪茄烟,自然均匀。The present invention also provides an application of Proline Maillard reactant for color enhancement and aroma enhancement in wrappers. The coating addition amount is 2-12%, which can improve the appearance and sensory quality of wrappers, harmonize with smoke, reduce The smoke is irritating and rich, making the appearance and color close to cigar smoke, natural and uniform.
本发明的有益效果是:The beneficial effects of the present invention are:
(1)脯氨酸与葡萄糖、木糖等还原糖按摩尔比2~6:1产生的美拉德反应,产物色泽为深棕黑色,糖含量较少,粘度减小,吸潮性降低,香气更丰富,品质提高;(1) Maillard reaction produced by proline and reducing sugars such as glucose and xylose in a molar ratio of 2 to 6:1, the color of the product is dark brown and black, the sugar content is less, the viscosity is reduced, and the moisture absorption is reduced. The aroma is richer and the quality is improved;
(2)脯氨酸与复合糖源-发酵咖啡豆提取物的美拉德反应产物,采用由龙胆二糖酶、内切纤维素酶、外切纤维素酶、中性和碱性蛋白酶、活性生香鲁氏干酵母等进行复合发酵咖啡豆提取液,起到复合协同作用,增酯增香且转化糖苷类香气物质,转化分解纤维素和蛋白质等不利于吸味的大分子细胞壁物质为葡萄糖、游离氨基酸、小分子物质等,更多地释放致香物质或其香味前体物,以及咖啡天然色素成分、抗氧化物等生物活性成分,再进行天然底物的美拉德反应,其中还可添加一定量的其他还原糖,制备脯氨酸增色增香美拉德反应物,具有咖啡烘烤香气,香气丰富,及具有一定的棕黑色着色能力;(2) The Maillard reaction product of proline and complex sugar source-fermented coffee bean extract, adopts gentiobiose, endocellulase, exocellulase, neutral and alkaline protease, Active aromatized Lushi dry yeast and other compound fermented coffee bean extracts have a compound and synergistic effect, increase esters, increase aroma, and transform glycoside aroma substances, transform and decompose macromolecular cell wall substances such as cellulose and protein that are not conducive to flavor absorption. Glucose, free amino acids, small molecular substances, etc., release more aroma-causing substances or their aroma precursors, as well as biologically active ingredients such as coffee natural pigment components, antioxidants, etc., and then carry out the Maillard reaction of natural substrates, of which A certain amount of other reducing sugars can also be added to prepare proline color-enhancing and flavor-enhancing Maillard reaction products, which have roasted coffee aroma, rich aroma, and certain brown-black coloring ability;
(3)脯氨酸与复合糖源的反应催化剂兼具调节pH值、促进反应、增加脯氨酸美拉德反应物的抗氧化稳定性的功能;(3) The reaction catalyst of proline and complex sugar source has the functions of adjusting pH value, promoting reaction, and increasing the antioxidant stability of proline Maillard reactant;
(4)该增色增香脯氨酸美拉德在再造烟叶及茄衣中的改善外观和感官质量的应用,很好地解决了当前工艺采用食品色素所带来的影响抽吸品质等问题,对再造烟叶和茄衣的外观和感官品质有提升作用,能协调烟气,中和烟气碱性,降低烟气刺激性,柔和烟气,丰富烟香,并使再造烟叶色泽自然均匀,茄衣呈现高贵典雅的深棕黑色,接近雪茄烟颜色。普通美拉德反应物的酸值,据报道,均在1以下,而本发明的脯氨酸美拉德反应物的酸值可达25.1,应用于再造烟叶及茄衣中,能起到中和烟气中的碱性,柔和烟气,降低烟气刺激性的作用。(4) The application of the color-enhancing and aroma-enhancing proline Maillard in reconstituted tobacco leaves and wrappers to improve the appearance and sensory quality has well solved the problems of affecting the smoking quality caused by the use of food coloring in the current process, It can improve the appearance and sensory quality of reconstituted tobacco leaves and wrappers, coordinate the smoke, neutralize the alkalinity of the smoke, reduce the irritation of the smoke, soften the smoke, enrich the aroma of the smoke, and make the color of the reconstituted tobacco leaves natural and uniform. The clothes are a noble and elegant dark brown-black color, which is close to the color of cigars. The acid value of common Maillard reactant, according to reports, is all below 1, and the acid value of proline Maillard reactant of the present invention can reach 25.1, is applied in reconstituted tobacco leaf and wrapper, can play a role And the alkalinity in the smoke, soften the smoke and reduce the irritation of the smoke.
本发明工艺条件简单温和,可直接使用现有生产设备,无需改造,所用的原料天然环保无害等优点,具有较大的工业应用前景。The process condition of the present invention is simple and mild, the existing production equipment can be directly used without modification, the raw materials used are natural, environmentally friendly and harmless, and have great industrial application prospects.
附图说明Description of drawings
图1是本发明制备的增色增香脯氨酸美拉德反应物样品的挥发性成分的总离子流色谱图;Fig. 1 is the total ion flow chromatogram of the volatile components of the color-enhancing and aroma-enhancing proline Maillard reactant sample prepared by the present invention;
图2是脯氨酸美拉德反应物对照的总离子图谱。Figure 2 is the total ion spectrum of the proline Maillard reactant control.
具体实施方式detailed description
下面将结合具体实施例,对本发明中的技术方案进行清楚、完整地描述。The technical solutions in the present invention will be clearly and completely described below in conjunction with specific embodiments.
实施例1Example 1
一种增色增香脯氨酸美拉德反应物的制备方法,具体包括如下步骤:A kind of preparation method of proline Maillard reactant of color-enhancing and aroma-enhancing, specifically comprises the following steps:
(1)原料准备;脯氨酸与糖源作为美拉德反应底物,本实施例中糖源为葡萄糖,按脯氨酸与葡萄糖的摩尔比3:1,反应催化剂为氨水,占美拉德反应底物质量的0.6%,水与反应底物的质量比为1.5:1;(1) Raw material preparation; Proline and sugar source are used as Maillard reaction substrate, and sugar source is glucose in the present embodiment, by the molar ratio of proline and glucose 3:1, and reaction catalyst is ammoniacal liquor, accounts for Maillard reaction. 0.6% of the mass of the reaction substrate, the mass ratio of water to the reaction substrate is 1.5:1;
(2)工业生产:先将水加入反应罐中,启动搅拌电机,加热至50℃,依次加入脯氨酸、葡萄糖,充分搅拌,直至完全溶解后,再加入氨水;反应过程中,设置美拉德反应罐工艺条件为温度98℃,搅拌电机保持开启状态,反应时间为6h;(2) Industrial production: first add water to the reaction tank, start the stirring motor, heat to 50°C, add proline and glucose in turn, and stir thoroughly until they are completely dissolved, then add ammonia water; during the reaction, set the Mela The process conditions of the German reaction tank are temperature 98°C, the stirring motor is kept on, and the reaction time is 6h;
(3)成品:反应结束后,待反应物在反应罐中自然冷却至35℃,过80目筛网过滤,以25+0.1公斤/桶的规格灌装,常温避光保存。(3) Finished product: After the reaction, the reactant is naturally cooled to 35°C in the reaction tank, filtered through an 80-mesh screen, filled with a specification of 25+0.1 kg/barrel, and stored at room temperature and protected from light.
本实施例还提供一种上述增色增香脯氨酸美拉德反应物在再造烟叶及茄衣中的应用,在再造烟叶进行涂布工序时添加,添加量为0.05%;在茄衣上应用,涂布添加量为8%,能改善再造烟叶及茄衣的外观和感官品质,与烟气协调,降低烟气刺激性,丰富烟气,柔和烟气,降低烟气的碱性,使外观色泽接近雪茄烟,自然均匀。This embodiment also provides an application of the above-mentioned proline Maillard reactant for color enhancement and aroma enhancement in reconstituted tobacco leaves and wrappers, which is added during the coating process of reconstituted tobacco leaves, and the addition amount is 0.05%; applied to wrappers , the coating addition amount is 8%, which can improve the appearance and sensory quality of reconstituted tobacco leaves and wrappers, coordinate with the smoke, reduce the irritation of the smoke, enrich the smoke, soften the smoke, reduce the alkalinity of the smoke, and make the appearance The color is close to cigar smoke, natural and uniform.
实施例2Example 2
一种增色增香脯氨酸美拉德反应物的制备方法,具体包括如下步骤:A kind of preparation method of proline Maillard reactant of color-enhancing and aroma-enhancing, specifically comprises the following steps:
(1)原料准备;按脯氨酸与发酵咖啡提取物的质量比为2:1来配置;反应催化剂为一定比例的氨水和维生素C,占上述脯氨酸与发酵咖啡提取物的质量的0.2%,水与反应底物的质量比为2.8:1;(1) Raw material preparation; configure according to the mass ratio of proline and fermented coffee extract as 2:1; the reaction catalyst is a certain proportion of ammonia water and vitamin C, accounting for 0.2% of the quality of the above-mentioned proline and fermented coffee extract %, the mass ratio of water and reaction substrate is 2.8:1;
(2)工业生产:先将水加入反应罐中,启动搅拌电机,加热至55℃,依次加入脯氨酸、发酵咖啡提取物,充分搅拌,直至完全溶解后,再加入催化剂氨水和维生素C(质量比为1:0.5);反应过程中,设置美拉德反应罐工艺条件为温度125℃,搅拌电机保持开启状态,反应时间为7h;(2) Industrial production: first add water to the reaction tank, start the stirring motor, heat to 55°C, add proline and fermented coffee extract in turn, stir thoroughly until completely dissolved, then add catalyst ammonia water and vitamin C ( The mass ratio is 1:0.5); during the reaction process, the process condition of the Maillard reaction tank is set to a temperature of 125°C, the stirring motor is kept on, and the reaction time is 7h;
(3)成品:反应结束后,待反应物在反应罐中自然冷却至38℃,过90目筛网过滤,以25+0.1公斤/桶的规格灌装,常温避光保存。(3) Finished product: After the reaction, the reactant is naturally cooled to 38°C in the reaction tank, filtered through a 90-mesh screen, filled with a specification of 25+0.1 kg/barrel, and stored at room temperature and protected from light.
所述的发酵咖啡豆提取物制备方法为:咖啡豆粗粉与水的质量比为1:25,由龙胆二糖酶、内切纤维素酶、外切纤维素酶、中性和碱性蛋白酶、活性生香鲁氏干酵母等进行复合发酵(活性生香鲁氏干酵母和酶均为食品级,龙胆二糖酶的酶活为1000u/g,其他酶的酶活均为10万u/g;质量比为0.3:0.5:0.5:0.5:0.5:1;复合酶和活性生香鲁氏干酵母占咖啡豆粗粉质量的0.2%)后,搅拌均匀,在pH 9,30℃条件下,温育发酵6h,95℃恒温水浴回流提取2次,合并滤液,减压浓缩至相对密度为1.15,为发酵咖啡豆提取物。The preparation method of the fermented coffee bean extract is as follows: the mass ratio of coffee bean coarse powder to water is 1:25, and the extract is prepared by gentiobiosaccharase, endocellulase, exocellulase, neutral and alkaline Compound fermentation with protease, active dry yeast of Roosevelt and other enzymes (both active dry yeast and enzymes are food grade, the enzyme activity of gentiobiase is 1000u/g, and the enzyme activity of other enzymes is 100,000 u/g; the mass ratio is 0.3:0.5:0.5:0.5:0.5:1; the compound enzyme and active Dried Yeast Lushii account for 0.2% of the mass of coffee bean meal), stir evenly, at pH 9, 30°C Under the conditions, incubate and ferment for 6 hours, reflux and extract twice in a constant temperature water bath at 95°C, combine the filtrates, concentrate under reduced pressure to a relative density of 1.15, and obtain fermented coffee bean extract.
该增色增香脯氨酸美拉德反应物在再造烟叶及茄衣中的应用,在再造烟叶进行涂布工序时添加,添加量为0.06%,在茄衣上应用,涂布添加量为9%,能改善再造烟叶及茄衣的外观和感官品质,与烟气协调,降低烟气刺激性,丰富烟香,具有咖啡烘烤香气,外观色泽接近雪茄烟,自然均匀。The application of the color-enhancing and aroma-enhancing proline Maillard reaction product in reconstituted tobacco leaves and wrappers is added during the coating process of reconstituted tobacco leaves, and the addition amount is 0.06%. When applied on wrappers, the coating addition amount is 9 %, can improve the appearance and sensory quality of reconstituted tobacco leaves and wrappers, harmonize with smoke, reduce the irritation of smoke, enrich the aroma of smoke, have the aroma of roasted coffee, and the appearance and color are close to cigars, natural and uniform.
实施例3Example 3
一种增色增香脯氨酸美拉德反应物的制备方法,具体包括如下步骤:A kind of preparation method of proline Maillard reactant of color-enhancing and aroma-enhancing, specifically comprises the following steps:
(1)原料准备;脯氨酸与复合糖源的按照质量比为3:1来配置,复合糖源为木糖与发酵咖啡豆提取物等质量比的复配物;反应催化剂为氨水、α-甲基苯甲醛,占美拉德反应底物质量的2%,水与反应底物的质量比为4.2:1;(1) Raw material preparation; proline and complex sugar source are configured according to a mass ratio of 3:1, and the complex sugar source is a compound of xylose and fermented coffee bean extract in an equal mass ratio; the reaction catalyst is ammonia water, α -tolualdehyde, accounts for 2% of Maillard reaction substrate quality, and the mass ratio of water and reaction substrate is 4.2:1;
(2)工业生产:先将水加入反应罐中,启动搅拌电机,加热至58℃,依次按一定比例加入脯氨酸、复合糖源,充分搅拌,直至完全溶解后,再加入催化剂;反应过程中,设置美拉德反应罐工艺条件为温度165℃,搅拌电机保持开启状态,反应时间为8h;(2) Industrial production: first add water to the reaction tank, start the stirring motor, heat to 58°C, add proline and complex sugar sources in a certain proportion in turn, stir fully, and then add the catalyst until it is completely dissolved; the reaction process , set the process conditions of the Maillard reaction tank at a temperature of 165°C, keep the stirring motor turned on, and the reaction time is 8 hours;
(3)成品:反应结束后,待反应物在反应罐中自然冷却至35~40℃,过100目筛网过滤,以25+0.1公斤/桶的规格灌装,常温避光保存。(3) Finished product: After the reaction, the reactant is naturally cooled to 35-40°C in the reaction tank, filtered through a 100-mesh screen, filled with a specification of 25+0.1 kg/barrel, and stored at room temperature and protected from light.
所述的发酵咖啡豆提取物制备方法为:咖啡豆粗粉与水的质量比为1:25,由龙胆二糖酶、内切纤维素酶、外切纤维素酶、中性和碱性蛋白酶、活性生香鲁氏干酵母等进行复合发酵(活性生香鲁氏干酵母和酶均为食品级,龙胆二糖酶的酶活为10000u/g,其他酶的酶活均为15万u/g;质量比为0.1:0.5:0.5:1:1:1;复合酶和活性生香鲁氏干酵母占咖啡豆粗粉质量的0.4%)后,搅拌均匀,在pH10,36℃条件下,温育发酵10h,93℃恒温水浴回流提取3次,合并滤液,减压浓缩至相对密度为1.18,为发酵咖啡豆提取物。The preparation method of the fermented coffee bean extract is as follows: the mass ratio of coffee bean coarse powder to water is 1:25, and the extract is prepared by gentiobiosaccharase, endocellulase, exocellulase, neutral and alkaline Compound fermentation with protease, active dry yeast of Roosevelt and other enzymes (both active dry yeast and enzymes are food grade, the enzyme activity of gentiobiase is 10000u/g, and the enzyme activity of other enzymes is 150,000 u/g; the mass ratio is 0.1:0.5:0.5:1:1:1; the compound enzyme and active Dried Yeast Rhododromyces account for 0.4% of the mass of the coffee bean meal), stir evenly, and put it under the conditions of pH10 and 36°C , incubated and fermented for 10 hours, refluxed and extracted three times in a constant temperature water bath at 93°C, combined the filtrates, concentrated under reduced pressure to a relative density of 1.18, and obtained fermented coffee bean extract.
本发明实施例还提供一种增色增香脯氨酸美拉德反应物在再造烟叶及茄衣中的应用,在再造烟叶进行涂布工序时添加,添加量为0.08%,在茄衣上应用,涂布添加量为11%,能改善再造烟叶及茄衣的外观和感官品质,与烟气协调,降低烟气刺激性,丰富香气,具有咖啡烘烤特征香气,使外观色泽接近雪茄烟,自然均匀。The embodiment of the present invention also provides an application of proline Maillard reactant for color enhancement and aroma enhancement in reconstituted tobacco leaves and wrappers, which is added during the coating process of reconstituted tobacco leaves, and the addition amount is 0.08%, and it is applied on wrappers , the coating addition amount is 11%, which can improve the appearance and sensory quality of reconstituted tobacco leaves and wrappers, harmonize with smoke, reduce the irritation of smoke, enrich the aroma, have the characteristic aroma of roasted coffee, and make the appearance and color close to cigars. Naturally even.
试验例1:应用的外观和感官效果对比评价Test Example 1: Comparative Evaluation of Application Appearance and Sensory Effects
将实施例1-3制备的增色增香脯氨酸美拉德反应物进行在再造烟叶及茄衣中的外观和感官评价,对照组为未施加美拉德反应物的再造烟叶或茄衣。The appearance and sensory evaluation of the color-enhancing and flavor-enhancing proline Maillard reactants prepared in Examples 1-3 in reconstituted tobacco leaves and wrappers were carried out, and the control group was reconstituted tobacco leaves or wrappers without Maillard reactants.
结果表明:本发明提供的脯氨酸美拉德反应物,在再造烟叶及茄衣中应用,能协调烟气,降低烟气刺激性,并丰富烟香,增加烘烤香气,中和烟气中的碱性,柔和烟气,并使外观色泽自然均匀,接近雪茄烟色泽。The results show that the proline Maillard reactant provided by the present invention, when applied in reconstituted tobacco leaves and wrappers, can harmonize the smoke, reduce the irritation of the smoke, enrich the aroma of the smoke, increase the roasted aroma, and neutralize the smoke Medium alkaline, soft smoke, and make the appearance of natural and uniform color, close to the color of cigar smoke.
表1.脯氨酸美拉德反应物在再造烟叶和茄衣中应用的外观和感官评价Table 1. Appearance and sensory evaluation of proline-Maillard reactants in reconstituted tobacco leaves and wrappers
试验例2:脯氨酸美拉德反应物的酸值对比Test Example 2: Acid Value Comparison of Proline Maillard Reactants
以紫外分光光度计来对比检测脯氨酸美拉德反应物及其对照的酸值,对照组a为脯氨酸:葡萄糖摩尔比为1:1的美拉德反应物,对照组b、对照组c为脯氨酸与复合糖源质量比为1:1的美拉德反应物,其他条件相同。Use a UV spectrophotometer to compare and detect the acid value of the proline Maillard reaction product and its control. The control group a is proline: the Maillard reaction product with a molar ratio of glucose of 1:1, and the control group b and control group Group c is a Maillard reactant with a mass ratio of proline to complex sugar source of 1:1, and other conditions are the same.
表2脯氨酸美拉德反应物的酸值The acid value of table 2 proline Maillard reactant
结果表明,经本发明的工艺条件生产的脯氨酸美拉德反应产物,酸值有极大提高,应用于再造烟叶及茄衣中,燃烧时,对烟气起到中和碱性的作用,柔和烟气,降低烟气刺激性。The results show that the acid value of the proline-Maillard reaction product produced by the process conditions of the present invention is greatly improved, and when applied to reconstituted tobacco leaves and wrappers, it can neutralize the alkalinity of the flue gas when burning , soft smoke, reduce smoke irritation.
试验例3:脯氨酸美拉德反应物挥发性成分的HS-SPME-GC/MS对比分析Test Example 3: HS-SPME-GC/MS Comparative Analysis of Volatile Components of Proline Maillard Reactants
称取脯氨酸美拉德反应物(脯氨酸与还原糖摩尔比2:1)样品和脯氨酸美拉德反应物对照(脯氨酸与还原糖的摩尔比为1:1,其他反应条件不变)各1g,分别置于15mL专用顶空萃取样品瓶中,选用100μm PDMS萃取头,以250℃条件下老化30min,再将萃取头插入装有脯氨酸-葡萄糖美拉德反应物的15mL专用顶空萃取样品瓶,在80℃萃取60min后,进行挥发性成分的GC/MS分析,分析结果如图1和图2所示。Take by weighing proline Maillard reactant (the molar ratio of proline and reducing sugar is 2:1) sample and proline Maillard reactant control (the molar ratio of proline and reducing sugar is 1:1, other Reaction conditions remain the same) each 1g, respectively placed in 15mL special headspace extraction vials, select 100μm PDMS extraction head, aged at 250°C for 30min, and then insert the extraction head into the proline-glucose Maillard reaction After extraction at 80°C for 60 minutes, GC/MS analysis of volatile components was carried out in a 15mL dedicated headspace extraction sample bottle of the compound. The analysis results are shown in Figure 1 and Figure 2.
GC/MS分析条件GC/MS analysis conditions
(1)色谱条件:柱初温50℃,保持2min,以8℃/min的速率升温到180℃,保持1min,再以18℃/min的速率升温到280℃,保持30min;载气为氦气(He,纯度99.99%),恒流模式,流速为1.0mL/min;分流进样方式,分流比1:10,无溶剂延迟;进样口温度250℃。(1) Chromatographic conditions: the initial column temperature is 50°C, keep for 2min, raise the temperature to 180°C at a rate of 8°C/min, keep for 1min, then raise the temperature to 280°C at a rate of 18°C/min, and keep for 30min; the carrier gas is helium Gas (He, purity 99.99%), constant flow mode, flow rate 1.0mL/min; split injection mode, split ratio 1:10, no solvent delay; inlet temperature 250 ° C.
(2)质谱条件:电离方式:EI源;电子能量:70eV;倍增管电压:1.2kV;离子源温度:230℃;四级杆温度:150℃;接口温度:280℃,传输线280℃;扫描范围:33-350m/z。使用NIST标准谱库进行检索分析,按峰面积归一化法计算化合物相对百分含量。(2) Mass spectrometry conditions: ionization method: EI source; electron energy: 70eV; multiplier tube voltage: 1.2kV; ion source temperature: 230°C; quadrupole temperature: 150°C; interface temperature: 280°C, transmission line 280°C; scanning Range: 33-350m/z. The NIST standard library was used for search and analysis, and the relative percentage of the compound was calculated according to the peak area normalization method.
表3脯氨酸-葡萄糖美拉德反应物挥发性成分的HS-SPME-GC/MS分析Table 3 HS-SPME-GC/MS analysis of volatile components of proline-glucose Maillard reaction product
从表3可以看出,采用HS-SPME-GC/MS方法从本发明的脯氨酸美拉德反应物(脯氨酸与还原糖摩尔比2:1)样品中共鉴定出76种挥发性成分,包括杂环化合物18种,酯类15种,醇类14种,烃类13种,酮类8种,酸类6种,烯类3种。按照面积归一化法来计算这76种挥发性成分的相对百分含量为73.39%,醛类含量最高,为42.94%,次高为酯类9.4%,醇类4.75%,烃类3.91,酮类2.74%,酸类2.28%,烯类0.77%,就单一物质而言,5-(1-哌啶)-2-呋喃甲醛最高,为35.38%,其次是5-羟甲基糠醛7.04%、邻苯二甲酸乙酸异丁酯3.23%、庚酸酐1.83%、(Z)-9-十六碳烯酸甲酯1.66%、十六醇1.39%、3-羟基-á-二氢突厥酮1.02%等。而脯氨酸美拉德反应物对照(脯氨酸与还原糖的摩尔比为1:1,)中共鉴定出59种挥发性成分,包括杂环化合物17种,酯类15种,醇类5种,烃类7种,酮类5种,酸类7种,酚类2种,按照面积归一化法来计算这59种挥发性成分的相对百分含量为63.23%,杂环化合物种类最多,单一物质而言,棕榈酸含量最高,达到12.60%,其次乙酸为8.45%,邻苯二甲酸乙酸异丁酯为7.21%,在本发明的脯氨酸美拉德反应物中,总挥发性成分的种类和相对百分含量增加,香气更丰富,且刺激性成分的种类和相对百分含量下降。As can be seen from Table 3, adopt the HS-SPME-GC/MS method to identify 76 kinds of volatile components altogether from the proline Maillard reactant (proline and reducing sugar molar ratio 2:1) sample of the present invention , including 18 heterocyclic compounds, 15 esters, 14 alcohols, 13 hydrocarbons, 8 ketones, 6 acids, and 3 alkenes. According to the area normalization method, the relative percentage of these 76 volatile components is 73.39%, the highest content of aldehydes is 42.94%, the second highest is esters 9.4%, alcohols 4.75%, hydrocarbons 3.91, ketones Alkenes 2.74%, Acids 2.28%, Alkenes 0.77%. As far as single substance is concerned, 5-(1-piperidine)-2-furfural is the highest at 35.38%, followed by 5-Hydroxymethylfurfural 7.04%, Isobutyl acetate phthalate 3.23%, heptanoic anhydride 1.83%, (Z)-9-hexadecenoic acid methyl ester 1.66%, cetyl alcohol 1.39%, 3-hydroxy-á-dihydroturkone 1.02% Wait. And proline Maillard reactant control (the molar ratio of proline and reducing sugar is 1:1,) identified altogether 59 kinds of volatile components, including 17 kinds of heterocyclic compounds, 15 kinds of esters, 5 kinds of alcohols There are 7 kinds of hydrocarbons, 5 kinds of ketones, 7 kinds of acids, and 2 kinds of phenols. According to the area normalization method, the relative percentage of these 59 volatile components is 63.23%, and the variety of heterocyclic compounds is the largest. , single substance, palmitic acid content is the highest, reaches 12.60%, secondly acetic acid is 8.45%, and phthalic acid isobutyl acetate is 7.21%, in proline Maillard reactant of the present invention, total volatility The types and relative percentages of ingredients increase, the aroma is richer, and the types and relative percentages of irritating ingredients decrease.
本发明的脯氨酸美拉德反应物的挥发性成分中,5-(1-哌啶)-2-呋喃甲醛是相对含量最高的物质;5-羟甲基糠醛是由葡萄糖等单糖化合物在高温等条件下脱水生成的具有呋喃环结构的醛类化合物,是美拉德反应的典型产物之一,广泛存在于食品中,对血管内皮细胞和小鼠四氯化碳肝损伤模型具有保护作用,也是2,5-呋喃二甲醛等的转化前体物质;辛酸奶酪味,腐败味,涩味,稀释后呈水果香气;柠檬烯是烷烃中阈值较低的一种“活性气味物质”,具有清新的柠檬香和柑橘香;β-广藿香烯是倍半萜类成分;庚酸丁酯呈草药和弱的生苹果似水果香味;2,6,10-三甲基十四烷等支链烷烃拥有一定的香气特征;月桂酸干果味、肉豆蔻酸等饱和脂肪酸,可赋予烟气一种腊味、脂味和柔和的吸味;月桂酸乙酯具有特有的花果香气,十六烷醇具有玫瑰香气;棕榈酸乙酯有脂肪味,腐败味,水果味,甜味等。所有这些挥发性成分构成了该脯氨酸-葡萄糖(2:1)美拉德反应物的特殊风味,能与烟气协调,柔和烟气,降低烟气刺激性,丰富烟香。Among the volatile components of the proline-Maillard reactant of the present invention, 5-(1-piperidine)-2-furfuraldehyde is the material with the highest relative content; 5-hydroxymethylfurfural is composed of monosaccharide compounds such as glucose Aldehyde compounds with furan ring structure, which are dehydrated under high temperature and other conditions, are one of the typical products of Maillard reaction, widely exist in food, and have protection for vascular endothelial cells and mouse carbon tetrachloride liver injury model It is also a precursor substance for the conversion of 2,5-furandicarbaldehyde, etc.; capry cheese, rancidity, astringency, fruity aroma after dilution; limonene is an "active odor substance" with a lower threshold in alkanes, which has Fresh lemon and citrus aroma; β-patchoulene is a sesquiterpene component; butyl heptanoate has herbal and weak raw apple-like fruity aroma; Paraffins have certain aroma characteristics; saturated fatty acids such as lauric acid and myristic acid can give the smoke a waxy, fatty and soft flavor; ethyl laurate has a unique floral and fruity aroma, cetane Alcohol has a rose aroma; ethyl palmitate has a fat, spoilage, fruity, sweet and so on. All these volatile components constitute the special flavor of the proline-glucose (2:1) Maillard reactant, which can coordinate with the smoke, soften the smoke, reduce the irritation of the smoke, and enrich the aroma of the smoke.
以上所述,仅为本发明的具体实施方式,但本发明的保护范围并不局限于此,任何属于本技术领域的技术人员在本发明揭露的技术范围内,可轻易想到的变化或替换,都应涵盖在本发明的保护范围之内。The above is only a specific embodiment of the present invention, but the scope of protection of the present invention is not limited thereto, any changes or substitutions that can be easily imagined by those skilled in the art within the technical scope disclosed in the present invention, All should be covered within the protection scope of the present invention.
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